反应详情

Trifluoroacetic acid (5.0 ml) was added to a solution of benzyl 4-{[(1-tetrahydro-2H-pyran-2-yl-1H-indazol-5-yl)amino]sulfonyl}-1-piperidinecarboxylate (500 mg, 1.00 mmol) in methylene chloride (50 ml) at room temperature and stirred for 2 hours. After the reaction solution was concentrated, a saturated aqueous sodium hydrogencarbonate solution was added thereto, followed by extraction with ethyl acetate. The organic layer was dried over anhydrous magnesium sulfate and distilled under reduced pressure to remove the solvent, and resulting residue was purified by a silica gel column chromatography (eluent: chloroform/methanol=50/1) to obtain benzyl 4-[(1H-indazol-5-ylamino)sulfonyl]piperidine-1-carboxylate (317 mg, 76%).

1. concentrationAfter the reaction solution was concentrated
2. additiona saturated aqueous sodium hydrogencarbonate solution was added
3. extractionfollowed by extraction with ethyl acetate
4. dry with materialThe organic layer was dried over anhydrous magnesium sulfate
5. distillationdistilled under reduced pressure
6. customto remove the solvent
7. customresulting residue
8. customwas purified by a silica gel column chromatography (eluent: chloroform/methanol=50/1)